RU2565660C2 - Method for production of smoking product sheet containing flavouring agent, smoking product sheet containing flavouring agent produced by said method and smoking product containing such sheet - Google Patents

Abstract

FIELD: tobacco industry.

SUBSTANCE: this invention relates to a method for production of a sheet containing a flavouring agent and applied for a smoking product, to such sheet containing a flavouring agent for a smoking product produced by such method and to a smoking product containing such sheet. Characterisation of the method for production of a sheet containing a flavouring agent for a smoking product is as follows: the method involves a stage of raw material suspension application onto the substrate where the suspension contains a polysaccharide containing at least either of carrageenan and gellan gum, a flavouring agent, an emulsifier and 70-95 wt % of water; the content of the flavouring agent is 100-1,000 wt % of the polysaccharide amount; the temperature in a colloidal state is equal to 60-90°C; there is also a stage of the applied raw material suspension active cooling till the sample temperature is equal to 0-40°C to produce gel and a stage of thermal drying involving gelated raw material heating and drying at the sample temperature equal to 70-100°C.

EFFECT: provision for a method for production of a sheet containing a flavouring agent for a smoking product within a shorter time where the sheet has a high content of the flavouring agent, a high yield of the flavouring agent and a good capacity to retain the flavouring agent after storage in case of introduction into a smoking product; the sheet has a good capacity o retain the flavouring agent after storage in case of introduction into a smoking product and can be produced within a shorter time.

13 cl, 5 dwg, 12 tbl, 11 ex

Description

FIELD OF THE INVENTION

The present invention relates to a method for producing a fragrance-containing sheet used for a smoking article, comprising a flavoring sheet for a smoking article obtained by this method, and containing a smoking article thereof.

BACKGROUND OF THE INVENTION

If a component that is a volatile aromatic substance such as menthol is added to the ground tobacco in the dissolved state, the aromatic component disappears during long-term storage and the aromatic effect is not retained. The following publications are devoted to solving this problem.

Patent documents 1 and 2 describe that an aromatic component is placed in a portion of a cigarette filter, the aromatic component being coated with a natural polysaccharide to suppress evaporation and disappearance of the aromatic component; and the coated aromatic component is crushed by squeezing it to release the flavor during smoking. Patent Document 3 describes that an aromatic component is placed in a portion of a cigarette filter, the aromatic component being coated with a water-soluble matrix such as dextrin to suppress evaporation and the disappearance of the aromatic component; and the water-soluble matrix is dissolved by the moisture of the smoke, which the smoker inhales, releasing the flavor at the time of smoking. Thus, when the aromatic component is placed in the filter part, which is the non-burning part of the cigarette, there is a delay until it smells, since the flavor is released by squeezing the filter part at the time of smoking or dissolving the water-soluble matrix with smoke moisture that the smoker inhales.

On the other hand, Patent Documents 4-6 give an example in which the aromatic component is placed in a burning portion, i.e., crushed tobacco or cigarette paper, into which tobacco is wrapped.

Patent Document 4 describes that a cigarette paper in which a tobacco filler is wrapped is coated with an aromatic material into which an aromatic component is introduced in a three-dimensional network of glucan molecules. The cigarette of Patent Document 4 has a good property of preserving the flavor, since the flavor component is fixed and kept included in the three-dimensional network of glucan molecules. However, the aromatic component is present in glucan molecules in a relatively small amount (20% by weight or less). Accordingly, in the case when it is required to add a sufficiently large amount of aromatic component, such as menthol, the amount in the mixture of aromatic material in the cigarette becomes high.

Patent Document 5 describes that a “stabilized aromatic substance that is stable up to 180 ° C” is obtained by mixing a liquid flavor with a carrageenan sol; dropping the mixture into an ionic solution (a solution containing potassium ions) to obtain a granular gel; and drying the gel in the air. However, the method of patent document 5 requires a long period of time and large production areas in order to obtain a large amount of material, since the granular gel is dried in air. In addition, this method requires the addition of a metal ion (gelling accelerator) in order to form a gel.

Patent Document 6 reports that a sheet containing an aromatic component coated with a polysaccharide gel is obtained by drying a suspension containing an aromatic component such as menthol and a polysaccharide; and the leaf is cut, and chopped pieces are added to the crushed tobacco. According to this report, a week is required for drying the suspension at 40 ° C.

As described above, various reports have been made as a method of suppressing the evaporation of an aromatic component, but there is still a need for a simple method for producing an aromatic material having an additionally improved ability to retain flavor after storage.

Background Documents

Patent document

Patent Document 1: Japanese Patent Application KOKAI Publication No. 64-27461.

Patent Document 2: Japanese Patent Application KOKAI Publication No. 4-75578.

Patent Document 3: International Publication No. 2009-157240.

Patent Document 4: Japanese Patent Application KOKAI Publication No. 9-28366.

Patent Document 5: Japanese PCT National Publication No. 11-509566.

Patent Document 6: International Publication No. 2009-142159.

SUMMARY OF THE INVENTION

The problem that will be solved by the present invention

An object of the present invention is to provide a method for producing a flavoring-containing sheet for a smoking article in a shorter time, where the sheet has a high flavoring content, a high flavoring yield and good ability to retain the flavoring after storage when introduced into the smoking article. Furthermore, it is an object of the present invention to provide a fragrance-containing sheet for a smoking article that has good ability to retain the flavor after storage when introduced into the smoking article, and can be obtained in a shorter time.

Ways to solve this problem

The authors of the present invention conducted research in order to solve these problems. As a result, they found that even if a high drying temperature is used, it is possible to obtain a flavoring sheet that has a high flavoring content and high flavoring yield and retains a high flavoring content even after storage, using carrageenan or gellan gum as a polysaccharide and cooling the sheet alone times before heat drying, and then drying it, upon receipt of a suspension of a raw material containing a polysaccharide, a flavoring agent and an emulsion containing a fragrance sheet by heat drying gator. Thus, they completed the present invention.

That is, according to one aspect of the present invention, there is provided a method for producing a fragrance-containing sheet for a smoking article, characterized in that it comprises:

the step of applying a slurry of raw material to a substrate, where the slurry contains a polysaccharide containing at least one of carrageenan and gellan gum, a flavoring agent, an emulsifier and 70-95% by weight of water, has a flavoring content of 100-1000% by weight relative to the polysaccharide and has a temperature of 60-90 ° C in a colloidal state;

the step of cooling the applied suspension of the crude material on the sample to a sample temperature of 0-40 ° C. to obtain a gel; and

the stage of thermal drying, including heating the gelled raw material and drying it at a sample temperature of 70-100 ° C.

According to a preferred embodiment, the emulsifier is 0.5-5% by weight of lecithin relative to the polysaccharide. Alternatively, in a preferred embodiment, the emulsifier is an ester selected from the group consisting of a fatty acid ester and glycerol, a fatty acid ester and polyglycerol, a fatty acid ester and sorbitol, a fatty acid ester and propylene glycol, and a fatty acid ester and sucrose.

According to a preferred embodiment, the polysaccharide is contained in a suspension of crude material at a concentration of 2-5% by weight.

According to a preferred embodiment, the flavor is menthol. According to a more preferred embodiment, the menthol content is in the range of 250-500% by weight relative to the polysaccharide.

According to another aspect of the present invention, there is provided a flavoring sheet for a smoking article, characterized in that it is obtained by the above method.

According to another aspect of the present invention, there is provided a smoking article comprising ground tobacco, characterized in that sliced pieces of the above flavoring sheet for a smoking article are mixed with ground tobacco.

The effects of the present invention

According to a method for producing a flavoring sheet for a smoking article of the present invention, it is possible to obtain a flavoring sheet for a smoking article in a shorter time, where the sheet has a high flavoring content, a high flavoring yield, and good ability to retain the flavoring after storage when introduced into the smoking article . In addition, the flavoring sheet for a smoking article of the present invention has good ability to retain flavor after storage when introduced into a cigarette, and can be obtained in a shorter time.

Brief Description of the Drawings

FIGURE 1 is a graph showing the menthol content of menthol-containing sheets after periods of storage.

FIGURE 2A is a graph showing a change in viscosity after lowering the temperature of an aqueous solution of gellan gum.

FIGURE 2B is a graph showing a change in viscosity after increasing the temperature of an aqueous solution of gellan gum.

FIGURE 3A is a graph showing the temperature of sample No. 1 during the heat-drying step.

FIGURE 3B is a graph showing the temperature of sample No. 2 during the heat-drying step.

FIGURE 3C is a graph showing the temperature of sample No. 3 during the thermal drying step.

FIGURE 3D is a graph showing the temperature of sample No. 4 during the process of thermal drying.

FIGURE 3E is a graph showing the temperature of sample No. 5 during the heat-drying step.

FIGURE 3F is a graph showing the temperature of sample No. 6 during the heat-drying step.

FIGURE 3G is a graph showing the temperature of sample No. 7 during the heat-drying step.

FIGURE 4A is a graph showing the effect of cooling on the menthol content after storage of menthol-containing sheets (comparative examples).

FIGURE 4B is a graph showing the effect of cooling on the menthol content after storage of menthol-containing sheets (examples of the present invention).

FIGURE 5 is a graph showing the relationship between the cooling temperature and the menthol content of menthol-containing sheets.

FIGURE 6 is a graph showing the relationship between the moisture content of menthol-containing sheets and the percent retention of menthol flavoring.

FIGURE 7A is a graph showing a change in viscosity after lowering the temperature of an aqueous carrageenan solution.

FIGURE 7B is a graph showing a change in viscosity after increasing the temperature of an aqueous carrageenan solution.

FIGURE 7C is a graph showing the temperature of a sample during the heat-drying step of a slurry of a crude material containing carrageenan as a polysaccharide.

FIGURE 7D is a graph showing the menthol content after storage of menthol containing sheets obtained using a suspension of raw material containing carrageenan as a polysaccharide.

FIGURE. 7E is a graph showing the temperature of a sample during a heat-drying step of a slurry of a crude material containing gellan gum as a polysaccharide.

FIGURE 7F is a graph showing the menthol content after storage of menthol-containing sheets obtained using a slurry of raw material containing gellan gum as a polysaccharide.

FIGURE 7G is a graph showing the change in viscosity after lowering the temperature of an aqueous pectin solution.

FIGURE 7H is a graph showing the change in viscosity after increasing the temperature of an aqueous pectin solution.

FIGURE 7I is a graph showing the temperature of a sample during the heat-drying step of a slurry of a crude material containing pectin as a polysaccharide.

FIGURE 7J is a graph showing the menthol content after storage of menthol containing sheets obtained using a suspension of raw material containing pectin as a polysaccharide.

FIGURE 7K is a graph showing the change in viscosity after lowering the temperature of an aqueous solution of konjak-glucomannan.

FIGURE 7L is a graph showing the change in viscosity after increasing the temperature of an aqueous solution of konjak-glucomannan.

FIGURE 7M is a graph showing the temperature of a sample during the heat-drying step of a slurry of a crude material containing konjac-glucomannan as a polysaccharide.

FIGURE 7N is a graph showing the menthol content after storage of menthol-containing sheets obtained using a slurry of raw material containing konjac-glucomannan as a polysaccharide.

FIGURE 8A is a graph showing the change in viscosity after lowering the temperature of an aqueous solution of carrageenan having different concentrations.

FIGURE 8B is a graph showing the change in viscosity after increasing the temperature of an aqueous solution of carrageenan having different concentrations.

FIGURE 8C is a graph showing the menthol content after storage of menthol-containing sheets obtained using raw material suspensions containing carrageenan at various concentrations.

FIGURE 8D is a graph showing changes in viscosity after lowering the temperature of an aqueous solution of gellan gum having different concentrations.

FIGURE 8E is a graph showing the change in viscosity after increasing the temperature of an aqueous solution of gellan gum having different concentrations.

FIGURE 8F is a graph showing the menthol content after storage of menthol containing sheets obtained using raw material suspensions containing gellan gum at various concentrations.

FIGURE 9A is a graph showing the menthol content after storage of menthol-containing sheets obtained using raw material suspensions containing carrageenan and menthol in various ratios.

FIGURE 9B is a graph showing the percent retention of menthol flavoring menthol-containing sheets obtained using raw material suspensions containing carrageenan and menthol in various ratios.

FIGURE 9C is a graph showing the yield of menthol-containing menthol sheets obtained using raw material suspensions containing carrageenan and menthol in various ratios.

FIGURE 9D is a graph showing the relationship between the proportion of menthol in the mixture and the menthol content of menthol-containing sheets (the case when the polysaccharide is carrageenan).

FIGURE 9E is a graph showing the relationship between the proportion of menthol in the mixture and the yield of menthol menthol-containing sheets (case when the polysaccharide is carrageenan).

FIGURE 9F is a graph showing the menthol content after storage of menthol-containing sheets obtained using raw material suspensions containing gellan gum and menthol in various ratios.

FIGURE 9G is a graph showing the percent retention of menthol flavoring menthol-containing sheets obtained using raw material suspensions containing gellan gum and menthol in various ratios.

FIGURE 9H is a graph showing the yield of menthol menthol-containing sheets obtained using raw material suspensions containing gellan gum and menthol in various ratios.

FIGURE 9I is a graph showing the relationship between the proportion of menthol in the mixture and the menthol content of menthol-containing sheets (the case when the polysaccharide is gellan gum).

FIGURE 9J is a graph showing the relationship between the proportion of menthol in the mixture and the yield of menthol menthol-containing sheets (the case when the polysaccharide is gellan gum).

FIGURE 10A is a graph showing the menthol content after storage of menthol-containing sheets obtained using raw material suspensions containing lecithin in various amounts in a mixture (weight ratio relative to polysaccharide) (case when the polysaccharide is carrageenan).

FIGURE 10B is a graph showing the relationship between the proportion of lecithin in a mixture and the menthol content of menthol-containing sheets (case where the polysaccharide is carrageenan).

FIGURE 10C is a graph showing the menthol content after storage of menthol-containing sheets obtained using raw material suspensions containing various amounts of lecithin in a mixture (weight ratio relative to polysaccharide) (case when the polysaccharide is gellan gum).

FIGURE 10D is a graph showing the relationship between the proportion of lecithin in the mixture and the menthol content of menthol-containing sheets (the case when the polysaccharide is gellan gum).

FIGURE 11A is a graph showing the effect of an emulsifier type on the menthol content of menthol-containing sheets (case when the polysaccharide is carrageenan).

FIGURE 11B is a graph showing the effect of an emulsifier type on the menthol content of menthol-containing sheets (case when the polysaccharide is gellan gum).

Embodiments of the present invention

The present invention will be explained below. The following explanation is intended to describe the present invention in detail, and is not intended to limit the present invention.

The flavoring contained in the flavoring sheet of the present invention is not limited, provided that it is used for a smoking article. Any type of flavoring may be used. Key examples of flavor include menthol, tobacco leaf extract; natural plant flavors (e.g. cinnamon, sage, herb, chamomile, kudzu (Pueraria lobata), hydrangea leaf, cloves, lavender, cardamom, cloves, nutmeg, bergamot, geranium, honey essence, rose oil, lemon, orange, cassia bark, caraway, jasmine, ginger, coriander, vanilla extract, mint, peppermint, cassia, coffee, celery, croton tree, sandalwood, cocoa, ylang-ylang, fennel, anise, licorice, St. John’s bread, extract prunes and peach extract), saccharides (e.g. glucose, f uctose, isomerized saccharide, and caramel), cocoa (e.g., powder and extract), esters (e.g., isoamyl acetate, linalyl acetate, isoamyl propionate and linalyl butyrate), ketones (e.g., menton, ionon, damaskenone and ethyl maltol), alcohols, e.g. , linalool, anethole and eugenol), aldehydes (e.g. vanillin, benzaldehyde and anisealdehyde), lactones (e.g. γ-undecalactone and γ-nonalactone); flavors of animal origin (e.g. musk, ambergris, cibetin and castoreum) and hydrocarbons (e.g. limonene and pinene). A flavoring agent that readily disperses in a solvent can be used by adding an emulsifier such as a hydrophobic flavoring and an oil soluble flavoring. This flavor can be used alone or in combination.

Further, the present invention will be explained by way of example where menthol is used as a flavoring.

1. Menthol-containing smoking article sheet

In one embodiment of the present invention, a menthol-containing sheet for a smoking article (hereinafter referred to as a “menthol-containing sheet”) is obtained by a process comprising:

the step of applying a slurry of raw material to a substrate, where the slurry contains a polysaccharide containing at least one of carrageenan and gellan gum, menthol and an emulsifier and 70-95% by weight of water, has a flavor content of 100-1000% by weight relative to the polysaccharide and has a temperature of 60-90 ° C in a colloidal state;

a step of cooling the applied slurry of the crude material to a sample temperature of 0-40 ° C. to obtain a gel; and

the stage of thermal drying, including heating the gelled raw material and drying it at a sample temperature of 70-100 ° C. The term "sample temperature" as used in the present invention refers to the temperature at the surface of a sample (i.e., a suspension or sheet).

(1) Obtaining a suspension of raw material

In the present invention, a suspension of raw material can be obtained by a method comprising: (i) a step of mixing a polysaccharide containing at least one of carrageenan and gellan gum with water and heating the mixture to obtain an aqueous polysaccharide solution; and (ii) a step of adding menthol and an emulsifier to the aqueous solution and mixing and emulsifying the mixture.

Specifically, step (i) can be carried out by adding small amounts of the polysaccharide to water, dissolving it in water with stirring. The heating temperature in the step may be 60-90 ° C, preferably 75-85 ° C. Stage (ii) can be carried out by any known method of emulsification using a homogenizer, since the suspension of the raw material has a viscosity of approximately 10,000 mPa · s (colloidal state), which does not interfere with emulsification, at the above heating temperature.

The polysaccharide is preferably contained in a suspension of crude material at a concentration of 2-5% by weight. For example, when 10 l of water is used as a solvent for a suspension of raw material, the suspension of raw material may contain 200-500 g of polysaccharide. More preferably, the polysaccharide is contained in a suspension of crude material at a concentration of 3-5% by weight (see example 10 below).

The composition of the suspension of raw material may be as follows:

for example, 500 g of polysaccharide, 500-5000 g of menthol and 50-500 ml of a solution containing 5% by weight of emulsifier, per 10 l of water.

The moisture content of the slurry of the crude material is 70-95% by weight, preferably 80-90% by weight.

The ratio (weight ratio) of polysaccharide and menthol in the suspension of raw material may be in the range of 1: 1-1: 10, preferably 1: 2.5-1: 5. That is, the proportion in the menthol mixture can be in the range of 100-1000% by weight relative to the polysaccharide, preferably 250-500% by weight relative to the polysaccharide (see example 11 below).

The suspension of raw material may contain either carrageenan or gellan gum as a polysaccharide, or may contain both of them. In addition, the polysaccharide may consist only of carrageenan and / or gellan gum, and another polysaccharide, such as tamarind gum, may be contained in addition to carrageenan and / or gellan gum. In this regard, another polysaccharide is contained in suspension with a fraction in the mixture, a smaller fraction in the mixture of carrageenan and gellan gum. As carrageenan, κ-carrageenan can be used.

In the present invention, the polysaccharide has the property of fixing the menthol micelle by coating it with gel formation upon cooling after heating. As for carrageenan and gellan gum, it was found that each of their aqueous solutions has particularly excellent characteristics of the sol-gel transition under the influence of temperature (see examples 4 and 9 below). That is, when an aqueous solution of carrageenan and an aqueous solution of gellan gum are cooled and a gel is formed, these solutions have the characteristics of being able to maintain a gel state, not easily returning to a colloidal state, even if the temperature is subsequently raised (see Figures 2B and 7B). Even if menthol coated with carrageenan or gellan gum is cooled once and then subjected to high temperature during the drying step, it is difficult to return the carrageenan or gellan gum coating to colloidal state due to these characteristics, and coated menthol can stably remain (see figures 7D and 7F). This ability is referred to in the present invention as “temperature sensitive sol-gel transition characteristics."

Thus, a polysaccharide having temperature-sensitive characteristics of the sol to gel transition has the advantage that it is possible to obtain excellent ability to retain flavor after storage by coating it with menthol, and also because there is no need to add metal ions (gelation accelerator), if temperature-sensitive characteristics of the transition of sol to gel for gelation are used.

In the present invention, l-menthol can be used as menthol.

In the present invention, a naturally occurring emulsifier, such as lecithin, specifically SUN LECITHIN A-1 (Taiyo Kagaku Co., Ltd.), can be used as an emulsifier.

When lecithin is used as an emulsifier, lecithin may be present in suspension in an amount of 0.5-5% by weight relative to the polysaccharide. When carrageenan is used as a polysaccharide, the added amount of lecithin is preferably 0.5-2% by weight relative to the polysaccharide. When gellan gum is used as a polysaccharide, the added amount of lecithin is preferably 0.5-5% by weight relative to the polysaccharide, more preferably 0.5-2% by weight relative to the polysaccharide (see example 12 below).

As an emulsifier, esters selected from the group consisting of a fatty acid ester and glycerol, a fatty acid ester and polyglycerol, a fatty acid ester and sorbitan, a fatty acid ester and propylene glycol and a fatty acid ester and sucrose can be used in addition to lecithin.

The fatty acid ester of glycerol includes, for example, fatty acid monoglycerides, such as monoglyceride monostearate or monoglyceride succinate; fatty acid ester of polyglycerol includes, for example, pentaglycerol monostearate; a fatty acid ester of sorbitan includes, for example, sorbitan monostearate; a fatty acid ester of propylene glycol includes, for example, propylene glycol monostearate; and the fatty acid and sucrose ester includes, for example, stearic acid and sucrose ester (see example 13 below). These emulsifiers may also be contained in the suspension in an amount of 0.5-5% by weight relative to the polysaccharide.

(2) Application of a suspension of crude material on a substrate

The resulting crude material suspension having a temperature of 60-90 ° C. is applied to the substrate.

A slurry of raw material can be applied by pressing a slurry of raw material onto a substrate by a gate or through a slot head. Any type of substrate can be used as a substrate, provided that the menthol-containing sheet obtained by dry molding can be removed from the substrate. For example, a polyethylene terephthalate (PET) film may be used (FE2001, FUTAMURA CHEMICAL CO., LTD.). The slurry of the raw material can be applied so that the thickness after drying becomes approximately 0.1 mm, which is equal to the thickness of standard ground tobacco.

(3) Cooling before dry molding the suspension

Upon receipt of the menthol-containing sheet of the present invention, the applied suspension of the crude material is cooled once before drying so that the suspension has a temperature that provides sufficient gelation of the suspension (40 ° C or less) and avoids the destruction of the emulsion by freezing (0 ° C or more), t. e., a temperature of 0-40 ° C, preferably 0-30 ° C, and more preferably 15-25 ° C. The suspension of raw material before cooling has a temperature of 60-90 ° C, preferably a temperature of 75-85 ° C and is in a colloidal state. Pre-cooling can be accomplished by blowing air or chilled air (e.g., 10 ° C) generated by a local air cooler (e.g., Suiden SS-25DD-1) over a applied suspension of raw material for 2-3 minutes. Alternatively, pre-cooling can be accomplished by contacting the applied slurry of the raw material with a pipe through which a cooling medium (e.g. 10 ° C) passes, generated by a cooling water generator (refrigerator, e.g. APISTE PCU-1600R) for 1-2 minutes. Alternatively, pre-cooling can be carried out by keeping the applied slurry of the crude material at room temperature.

As shown in examples 4 and 9 below, when the polysaccharide solution described above is cooled and a gel forms, the solution is able to maintain a gel state without easily returning to a colloidal state, even at a temperature of transition to a gel, even if the temperature is subsequently raised. The above property is used in the present invention, and pre-cooling is carried out before drying the suspension of raw material. As a result, the polysaccharide contained in the slurry of the raw material after preliminary cooling is difficult to convert to sol, even if the temperature is raised during drying, and the menthol coated with the polysaccharide is difficult to evaporate. This is demonstrated in the present invention.

When a suspension of the raw material is applied to the substrate and then cooled, the advantage is that the applied suspension of the raw material is difficult to deform, even if it is exposed to high temperatures in the subsequent drying step.

The effect of cooling on the fragrance retention property after storage of the fragrance-containing sheet is shown in Example 6 below (Figure 4B). Lower cooling temperatures result in a higher menthol content, as demonstrated in Example 7 below (FIG. 5).

(4) Dry suspension molding

Thermal drying of the applied and cooled slurry of raw material can be carried out with any type of thermal drying, such as drying with hot air or drying with thermal radiation in the infrared region of the spectrum. Further, the "drying" of a suspension of raw material is called simply "drying."

In the present invention, drying a suspension of raw material includes drying by heating a cooled suspension of raw material at a sample temperature of 70-100 ° C. Preferably, the temperature of the sample is 100 ° C. or less during the total drying time. If the suspension is dried at the above sample temperature, the menthol evaporation can be suppressed, and the menthol-containing sheet can be obtained in a shorter time.

The term "sample temperature" refers to the temperature at the surface of a sample (i.e., a suspension or sheet). The term "total drying time" refers to the period of heating in a heated dryer. The total drying time is usually 20 minutes or less, preferably 7-20 minutes, more preferably 10-18 minutes.

In the present invention, the temperature of the sample may be less than 70 ° C during the drying step. However, in order to shorten the drying time, it is preferable to shorten the period when the temperature of the sample is less than 70 ° C. In the present invention, the temperature of the sample may exceed 100 ° C during the drying step. However, in order to stably maintain a flavoring agent, such as a menthol flavoring, it is preferable to shorten the period when the temperature of the sample exceeds 100 ° C. Therefore, the drying of the suspension of raw material can preferably be carried out by drying the cooled suspension of raw material at a sample temperature of 70-100 ° C for more than half the total drying time. Preferably, the temperature of the sample is 100 ° C or less during the total drying time. More preferably, the drying of the suspension of the raw material can be carried out by drying the cooled suspension of the raw material at a sample temperature of 70-100 ° C for a total drying time.

However, immediately after the start of thermal drying, the temperature of the sample in the heated dryer is average between the pre-cooling temperature and the required temperature of the sample (70 ° C) and does not reach the required temperature of the sample. When expressed as “at a sample temperature of 70-100 ° C for the total drying time”, the term “total drying time” refers to the total drying time, excluding the initial period when the temperature of the sample is in the middle of rising to the desired temperature of the sample. For example, in Example 5 (Figures 3A-3G) below, the temperature of the sample is in the middle of the rise to the desired temperature of the sample within about 1 minute after the start of heat drying. Thus, the initial period is excluded from the "total drying time" when expressed as "at a sample temperature of 70-100 ° C during the total drying time".

Preferably, the suspension of the raw material can be dried by drying the suspension of the raw material so as to obtain a sheet form having a moisture content of less than 10% over a total drying time of 20 minutes or less.

Example 5 below (3D-3G figures) shows that when a slurry of raw material was dried at the temperature of the sample above, the sheet obtained by drying can acquire good ability to retain flavor after storage.

Next, the case of drying with hot air will be explained. In the case of drying with hot air, in order to maintain the sample temperature of 70-100 ° C, the suspension of the raw material is preferably dried with hot air having a temperature of 100 ° C or more during the initial drying, and then with hot air having the same temperature as during initial drying or a temperature lower than the temperature of the initial drying (preferably 70 ° C or more and less than 100 ° C). Accordingly, it is possible to suppress the increase in sample temperature during subsequent drying. For example, you can keep the temperature of the sample so that it does not exceed 100 ° C during the total drying time.

In the present invention, it is possible that the obtained menthol-containing sheet has a high menthol content and a high menthol yield and maintains a high menthol content after storage, when the suspension of the crude material is cooled, even if the subsequent drying step involves a drying method in which the temperature of the sample reaches 70-100 ° C (e.g., drying at high temperature with hot air having a temperature of 100 ° C or more).

In the case of drying with hot air, the temperature of the hot air may be a constant temperature during the entire period of the drying stage or may vary during the drying stage. When the temperature of the hot air changes, it is preferable to dry the suspension of the raw material by first drying it at high temperature with hot air having a temperature of 100 ° C or more, and then drying it at a low temperature with hot air having a temperature of less than 100 ° C. The term “initial drying” as used in the present invention means the first drying in the drying step of hot air having a temperature of 100 ° C or more, and the term “subsequent drying” means drying after initial drying with hot air having a low temperature of less than 100 ° C. Thus, if the initial drying with hot air having a high temperature is carried out in combination with subsequent drying with hot air having a low temperature, it is preferable that the temperature of the sample does not become too high. In the case of drying with hot air, the drying temperature is the same as the temperature of hot air.

More preferably, the slurry of raw material can be dried so that a sheet form having a moisture content of less than 10% is obtained over a total drying time of 20 minutes or less, by initial drying at a hot air temperature of 100 ° C or more for a quarter or more the total drying time, and then conducting subsequent drying at a hot air temperature of less than 100 ° C for a quarter or more of the total drying time.

Thus, if the initial drying with hot air having a high temperature is carried out in combination with subsequent drying with hot air having a low temperature, the temperature increase during subsequent drying can be suppressed. For example, you can maintain the temperature of the sample so that it does not exceed 100 ° C.

Accordingly, it is possible that the menthol-containing sheet of the present invention has a high menthol content after receiving the sheet and also maintains a high menthol content after storage (see sample No. 4 of example 1, sample No. 5 of example 2 and sample No. 6 of example 3 below).

When the suspension of the raw material is dried by drying with hot air, the initial drying can be carried out, for example, with hot air having a temperature of 100-130 ° C for 4-6 minutes, and the subsequent drying can be carried out, for example, with hot air having a temperature of 70 ° C or more and less than 100 ° C for 4-6 minutes. The volume of hot air can be set, for example, to 3-20 m / s. The total drying time is usually 20 minutes or less, preferably 7-20 minutes, more preferably 10-18 minutes.

The conditions for initial drying and subsequent drying (temperature, duration and volume of air) can be suitably set, for example, in the above range. For example, initial drying is carried out at a hot air temperature of 100-130 ° C before moisture evaporates from the surface of the slurry of the raw material and a sufficient film forms on the surface of the slurry. Then, the hot air temperature is immediately replaced by a temperature in the range of 70 ° C or more and less than 100 ° C, and subsequent drying can be carried out.

The temperature of the hot air during the initial drying process can be constant, or it can be changed so as to reduce it to a range of 100-130 ° C. The temperature of the hot air during the subsequent drying process can be constant, or it can be changed so as to lower it to a range of 70 ° C or more and less than 100 ° C. For example, the hot air dryer used in the examples below has three drying chambers, and each sample is moved in order through the first, second, and third chamber by a belt conveyor. Thus, the first and second chambers can be used for initial drying at the same or different temperatures (100 ° C or more), and the third chamber can be used for subsequent drying (less than 100 ° C). Alternatively, the first chamber is used for initial drying (100 ° C or more), and the second and third chambers can be used for subsequent drying at the same or different temperatures (less than 100 ° C).

In the present invention, drying is carried out until the menthol-containing sheet is sufficiently dried so that the sheet can be easily removed from the substrate and can be cut in a subsequent cutting step. Specifically, drying is carried out until the moisture content of the menthol-containing sheet becomes less than 10% by weight, preferably 3-9% by weight, more preferably 3-6% by weight (see Example 8 below). The term “moisture content” as used in the present invention means a value measured according to the measurement method described in the following examples.

Immediately upon receipt, the menthol content of the menthol-containing sheet of the present invention is preferably 45% by weight or more, more preferably 55-75% by weight. After storage (at 50 ° C. for 30 days), the menthol content of the menthol-containing sheet of the present invention is preferably 45% by weight or more, more preferably 48-63% by weight. The term “menthol content” as used in the present invention means a value measured according to the measurement method described in the following examples.

2. Product for smoking

The menthol-containing sheet of the present invention is cut, for example, to a size equal to the size of the standard ground tobacco and thus the sliced pieces can be mixed with the ground tobacco for the smoking article. Sliced pieces of menthol-containing sheet can be added in an amount of 2-10 g per 100 g of ground tobacco. The chopped pieces of the menthol-containing sheet are preferably distributed in crushed tobacco and mixed with it.

The menthol-containing sheet of the present invention can be mixed with ground tobacco for any type of smoking article, for example a burning type smoking article in which a smoker smells smoke by burning tobacco leaves, in particular a cigarette. In particular, the menthol-containing sheet of the present invention can be mixed with crushed tobacco of a cigarette containing a cigarette rod that contains crushed tobacco and cigarette paper wrapped in tobacco.

Examples

[Example 1]

(1) Obtaining a suspension of raw material (10 L scale)

water 10 l

gellan gum (KELCOGEL, San-Ei Gen F.F.I., Inc.) 150 g

tamarind gum (BISTOP D-2032, San-Ei Gen F.F.I., Inc.) 150 g

Lecithin (SUN LECITHIN A-1, Taiyo Kagaku Co., Ltd.) 120 ml (5% aqueous solution)

menthol (Takasago International Corporation.) 1500 g

Water (10 L) was kept at 80 ° C, and gellan gum (150 g) and tamarind gum (150 g) were added and dissolved in small portions so that no lumps formed (required time: approximately 20 minutes) while stirring with a mixer (PRIMIX TK AUTO MIXER Model 40 / equipped with a rotor for stirring the solution / 2000 rpm), and menthol (1500 g) was added.

The rotating blade stirrer was replaced with a homogenizer (PRIMIX T.K. AUTO MIXER Model 40 / equipped with a rotor-stator head / 4000 rpm), and the mixture was emulsified for 10 minutes. Then, lecithin (120 ml of 5% aqueous solution) was added to the mixture, followed by emulsification for 10 minutes, obtaining a suspension of crude material.

(2) Dry Forming

The resulting suspension of the crude material was applied to the film base through a slit head. After that, the cold air generated by the local cooler (Suiden SS-25DD-1) (10 ° C) was blown over the suspension of raw material for 2-3 minutes so as to cool the suspension of raw material to about 20 ° C. After that, it was dried with hot air by transferring it to a conveyor belt in a hot air dryer to obtain a menthol-containing sheet in film form. The details of the experiment will be described below.

Slit head: vertical slit head (which is heated to 60 ° C and remains heated), 900 μm thick and 20 cm wide

Film base: PET film (which is corona treated), 50 μm thick

Hot Air Dryer: A type of hot air dry forming machine having the following configuration

Drying compartment: three chambers (length of each zone: 2.5 m, total length: 7.5 m)

Air Volume and Hot Air Shape:

First chamber: perforated plate, air volume: 5 m / s.

Second chamber: perforated plate, air volume: 10 m / s.

Third chamber: injector for translation into a "floating state", air volume: 20 m / s.

In the first and second chambers, hot air was blown over the menthol-containing sheet, which is supplied on the tape, through a perforated plate, which functions as a plate for controlling flow. In the third chamber, hot air was blown over the menthol-containing sheet, which was supplied in a “floating state” along with the film base of the upward and downward ventilation.

The drying conditions with hot air were changed as described in table 1 below, obtaining menthol-containing sheets of samples No. 1-4. The temperature shown in the table is the temperature of the hot air. The drying time was set so that the menthol-containing sheet was sufficiently dried, it could be easily removed from the film base, and it could be cut in a subsequent cutting step. The moisture content of menthol-containing sheets obtained in this example was approximately 3%.

(3) Study of the dry state of menthol-containing leaf

The moisture content of the menthol-containing sheet was measured by GC-TCD as follows.

0.1 g of a menthol-containing sheet (cut into 1 × 10 mm pieces) was weighed. 10 ml of methanol (a new reagent of a special quality or superior quality was dosed under conditions without exposure to air to eliminate the effect of water absorption from the air) was added to the chopped pieces in a 50 ml closed container (tube with a screw cap), followed by shaking at 200 rpm for 40 minutes. The resulting mixture was left overnight, shaken again at 200 rpm for 40 minutes and left. The supernatant was used as a measurement solution (without dilution for GC measurement).

The measurement solution was analyzed by GC-TCD and quantified using a calibration curve method.

GC-TCD; 6890 gas chromatograph obtained by Hewlett Packard

Speaker; HP Polapack Q (packed column) 20.0 mL / min continuous flow mode

Introduction; 1.0 μl

Inlet valve; EPC inlet valve for purging packed column

Heating device; 230 ° C

Gas; He

Total flow; 21.1 ml / min

Dryer; 160 ° C (holding for 4.5 minutes) → (60 ° C / min) → 220 ° C (holding for 4.0 minutes)

Detector; TCD detector

Comparison Gas (He)

flow rate; 20 ml / min

Auxiliary gas (He) 3.0 ml / min

Signal transfer rate; 5 Hz

The concentration of the solutions of the calibration curve; six points 0, 1, 3, 5, 10 and 20 [mg-H ₂ O / 10 ml]

(4) Measurement of menthol content in menthol-containing sheet

The menthol content in menthol-containing sheets was measured by GC-FID in the following manner.

0.1 g of a menthol-containing sheet (cut into 1 × 10 mm pieces) was weighed. 10 ml of methanol (a new reagent of a special quality or superior quality was dosed under conditions without exposure to air to eliminate the effect of water absorption from the air) was added to the chopped pieces in a 50 ml closed container (tube with a screw cap), followed by shaking at 200 rpm for 40 minutes. The resulting mixture was left overnight, shaken again at 200 rpm for 40 minutes and left. The supernatant was used as a measurement solution (10-fold dilution with methanol for GC measurement).

The measurement solution was analyzed by GC-FID and quantified using a calibration curve method

GC-FID; 6890N Agilent Gas Chromatograph

Speaker; DB-WAX 30 m × 530 μm × 1 μm

5.5 psi constant pressure mode (speed; 50 cm / s)

Introduction; 1.0 μl

Inlet valve; Spritless mode 250 ° C 5.5 psi

Dryer; 80 ° C → (10 ° C / min) → 170 ° C (holding for 6.0 minutes) [maximum 220 ° C]

Detector; FID detector 250 ° C (H2; 40 ml / min air; 450 ml / min)

Signal transfer rate; 20 Hz

The concentration of the solutions of the calibration curve; eight points 0, 0.01, 0.05, 0.1, 0.3, 0.5, 0.7 and 1.0 [mg-menthol / ml]

The menthol content (mg) of the obtained menthol-containing sheet and the menthol content (mg) of the menthol-containing sheet stored under forced conditions were measured. The results are shown in table 1 as "initial menthol content (%)" and "menthol content after storage (%)".

The initial menthol content (%) = {measured value of the menthol content (mg) / weight of the sheet containing menthol (mg)} × 100

Menthol content after storage (%) = {measured value of menthol content (mg) / weight of menthol-containing sheet (mg)} × 100

Forced conditions were as follows.

About 5 g of a menthol-containing sheet (cut into 1 × 10 mm pieces) was placed in an open container and stored for a maximum of 30 days in a thermostat (oven DX600, Yamato Scientific Co., Ltd.) set at 50 ° C.

The percentage of menthol flavoring was calculated from the menthol content using the following equation, and the ability to retain the flavor of the menthol-containing sheet was evaluated.

The percentage of menthol flavoring (%) = {(menthol content after storage) / (initial menthol content)} × 100

(5) Results

The menthol-containing sheets of samples No. 1-4 were obtained with a hot air dryer under the hot air drying conditions described in Table 1. The moisture content and initial menthol content of menthol-containing sheets were measured according to the above method. The results are shown in Table 1. The menthol content of a sheet stored for 30 days is shown in Table 1. The menthol content of a sheet stored for 7 days, 14 days, and 30 days is shown in the figure. 1. The position numbers 1-7 in figure 1 represent samples No. 1-7.

Table 1 Sample No. one 2 3 four Hot Air Drying Conditions First camera 70 ° C • 4 min 120 ° C • 2 min 70 ° C • 20 min 120 ° C • 2.5 min Second camera 80 ° C • 4 min 130 ° C • 2 min 70 ° C • 20 min 120 ° C • 2.5 min Third camera 120 ° C • 4 min 176 ° C • 2 min 70 ° C • 20 min 70 ° C • 2.5 min Belt speed 0.6 m / min 1.3 m / min 0.13 m / min 1,0 m / min Moisture contents 3.1% 3.2% 3.1% 3.4% Initial Menthol Content 81.5% 62.4% 75.8% 75.7% Menthol Content After Storage 13.6%
(in 20 days) 29.2%
(after 30 days) 59.2%
(after 30 days) 62.4%
(after 30 days) Percentage of flavoring 17% 47% 78% 82%

Sample No. 1

When a slurry of raw material is applied and dried with a hot air dryer to obtain a sheet form, in many cases, hot air drying is started at a low temperature (approximately 70 ° C) so that a surface does not form in the first part of the drying, and hot air drying is continued at high temperature (approximately 120 ° C) so as to achieve complete drying in the second half of the drying. According to this drying method, a menthol-containing sheet of sample No. 1 was obtained, and as a result, a sufficiently dried sample (moisture content: 3.1%) can be obtained for a total drying time of 12 minutes. The "initial menthol content" after receiving the sheet was up to 81.5%, but the "menthol content after storage" after storage (for 20 days) under forced conditions was only 13.6%. Thus, the sheet of sample No. 1 has problems with the property of preservation of the flavor after storage.

Sample No. 2

In sample No. 2, high drying temperatures were used to make the drying time shorter than the duration of example No. 1. As a result, in sample No. 2, a sufficiently dried sample (moisture content: 3.2%) can be obtained for the total duration drying 6 minutes. The "initial menthol content" after receiving the sheet was up to 62.4%, but the "menthol content after storage" after storage (within 30 days) under forced conditions was only 29.2%. Thus, the sheet of sample No. 2 has problems with the property of preservation of the flavor after storage.

Sample No. 3

In sample No. 3, the temperature of the hot air was set to 70 ° C during the entire period of the drying stage. As a result, in sample No. 3, a sufficiently dried sample (moisture content: 3.1%) can be obtained for a total drying time of 60 minutes. The "initial menthol content" after receiving the sheet was up to 75.8%, and the "menthol content after storage" after storage (within 30 days) under forced conditions was up to 59.2%. Thus, both the ability to retain flavor after sheet production and the ability to retain flavor after storage were excellent. However, the required drying time was up to 60 minutes.

Sample No. 4

In sample No. 4, in contrast to samples No. 1 and 2, in which low-temperature drying was replaced by high-temperature drying, the initial drying (in the first and second chambers) was carried out with hot air at high temperature (120 ° C), and subsequent drying (in the third chamber) was carried out with hot air at a low temperature (70 ° C). In sample No. 4, the total drying time was as short as 7.5 minutes, however, it is possible to obtain a sufficiently dried sample (moisture content: 3.4%). The "initial menthol content" after receiving the sheet was up to 75.7%, and the "menthol content after storage" after storage (within 30 days) under forced conditions was up to 62.4%. Thus, both the ability to retain flavor after sheet production and the ability to retain flavor after storage were excellent. The results show that it is possible to obtain a sheet having excellent ability to retain flavor in a relatively short period of time if the initial high-temperature drying and subsequent low-temperature drying are used.

[Example 2]

The menthol-containing sheet of sample No. 5 was obtained by a method similar to that of example 1, except that the suspension was dried under the hot air drying conditions described in table 2 below, and the moisture content and menthol content were measured. The results are shown in table 2.

table 2 Sample No. 5 Hot Air Drying Conditions First camera 120 ° C • 4 min [Injector to translate into a "floating state" 20 m / s] Second camera 70 ° C • 4 min [Injector 20 m / s] Third camera 70 ° C • 4 min [Injector 10 m / s]

Belt speed 0.6 m / min Moisture contents 3.1% Initial Menthol Content 72.7% Menthol Content After Storage 58.5% Percentage of flavoring 80%

In sample No. 5, the volume of hot air was increased compared to the volumes of samples No. 1-4. In the first chamber, hot air was blown over the menthol-containing sheet, which was supplied in a "floating state" by upward and downward ventilation. In the second and third chambers, hot air was blown over the menthol-containing sheet, which was supplied by ventilation on the tape.

In sample No. 5, the initial drying (in the first chamber) was carried out with hot air at a high temperature (120 ° C) for 4 minutes and the subsequent drying (in the second and third chambers) was carried out with hot air at a low temperature (70 ° C) for 8 minutes. In sample No. 5, a sufficiently dried sample (moisture content: 3.1%) can be obtained for a total drying time of 12 minutes. The "initial menthol content" after receiving the sheet was up to 72.7%, and the "menthol content after storage" after storage (within 30 days) under forced conditions was up to 58.5%. Thus, both the ability to retain flavor after sheet production and the ability to retain flavor after storage were excellent. The results show that it is possible to obtain a sheet having excellent ability to retain flavor in a relatively short period of time if the initial high-temperature drying and subsequent low-temperature drying are used.

[Example 3]

Menthol-containing sheets of samples No. 6 and 7 were obtained by a method similar to that of example 1, except that the suspension was dried using a hot air dryer containing four drying chamber chambers under the hot air drying conditions described in table 3 below, and the moisture content was measured and menthol content. The results are shown in table 3.

Table 3 Sample No. 6 7 Hot Air Drying Conditions First camera 110 ° C • 2.2 min
[Injector, 10 m / s] 100 ° C • 2.2 min
[Injector, 10 m / s] Second camera 100 ° C • 2.2 min
[Injector, 10 m / s] 100 ° C • 2.2 min
[Injector, 10 m / s] Third camera 100 ° C • 2.2 min
[Injector, 10 m / s] 100 ° C • 2.2 min
[Injector, 10 m / s] Fourth camera 80 ° C • 2.2 min
[Injector, 10 m / s] 100 ° C • 2.2 min
[Injector, 10 m / s] Belt speed 0.9 m / min 0.9 m / min Moisture contents 5% 4.9% Initial Menthol Content 63.5% 61.9% Menthol Content After Storage 59.9%
(after 30 days) 60.8%
(after 30 days) Percentage of flavoring 94% 98%

In samples No. 6 and 7, menthol-containing sheets were prepared using a hot air dryer having four drying chamber chambers.

In sample No. 6, the initial drying (in the first and third chambers) was carried out with hot air at high temperature (110 ° C → 100 ° C) for 6.6 minutes, and the subsequent drying (in the fourth chamber) was carried out with hot air at low temperature ( 80 ° C) for 2.2 minutes. In sample No. 6, a sufficiently dried sample (moisture content: 5%) can be obtained for a total drying time of 8.8 minutes. The "initial menthol content" after receiving the sheet was up to 63.5%, and the "menthol content after storage" after storage (within 30 days) under forced conditions was up to 59.9%. Thus, both the ability to retain flavor after sheet production and the ability to retain flavor after storage were excellent. The results show that it is possible to obtain a sheet having excellent ability to retain flavor in a relatively short period of time using the initial high-temperature drying and subsequent low-temperature drying, although the hot air temperature is subsequently reduced from 110 ° C to 100 ° C during the initial drying.

In sample No. 7, the hot air temperature was set to 100 ° C during the entire period of the drying stage, regardless of the initial drying and subsequent drying. In sample No. 7, subsequent drying at a low temperature was not used, but it is assumed that the temperature of the sample does not become too high during the drying of the suspension due to the presence of moisture in the sample, similarly to samples No. 4-6. Specifically, in sample No. 7, a sufficiently dried sample (moisture content: 4.9%) can be obtained for a total drying time of 8.8 minutes. The "initial menthol content" after receiving the sheet was up to 61.9%, and the "menthol content after storage" after storage (within 30 days) under forced conditions was up to 60.8%. Thus, both the ability to retain flavor after sheet production and the ability to retain flavor after storage were excellent. The results show that it is possible to obtain a sheet having excellent ability to retain flavor in a relatively short period of time, similar to the cases of samples No. 4-6, although the same temperature of hot air (100 ° C) was used during the entire period of the drying stage.

[Example 4]

In this example, temperature-sensitive characteristics of the transition of the sol to the gel of a polysaccharide solution (suspension) were investigated.

Water 0.1 L

Gellan Gum (KELCOGEL, San-Ei Gen F.F.I., Inc.) 5 g

Water (0.1 L) was kept at 70 ° C, and gellan gum (5 g) was added and dissolved in it in small portions so that no lumps formed while stirring it using a high-performance DMM mixer (ATEC Japan Co., Ltd.) and a polysaccharide solution (suspension) was obtained.

The temperature of the resulting suspension (70 ° C) was lowered to 25 ° C for approximately 900 seconds (0.05 ° C / s). Then, the temperature was raised to 70 ° C for approximately 900 seconds. Figures 2A and 2B show how the viscosity (fluidity) of the suspension changed with temperature.

As shown in figure 2A, if the temperature of the suspension was reduced to 25 ° C (cooling), the viscosity was low up to a temperature of 50 ° C (fluidity was high). However, the viscosity unexpectedly increased at 40 ° C or less (gel effect). If the temperature of the obtained gel was increased, the gel did not easily return to the colloidal state, even if the temperature exceeded the gelation temperature (40 ° C), as shown in Figure 2B. Thus, the gel state was maintained up to a very high temperature.

The result shows that when the polysaccharide-containing suspension is cooled and a gel is formed, it is difficult to return the suspension to a colloidal state, even if the temperature is subsequently raised, and thus a gel state can be maintained. The above property of the polysaccharide is used in the present invention, and pre-cooling is carried out before drying the suspension of crude material. As a result, it is expected that the polysaccharide contained in the slurry of the raw material after pre-cooling is difficult to sol, even if the temperature was raised during drying, and the menthol coated with the polysaccharide is difficult to evaporate.

[Example 5]

In this example, sheets of samples No. 1-7 were obtained as described in examples 1-3, and the temperature of the samples was measured during the drying stage. Regarding the conditions for drying hot air samples No. 1-7, you can refer to tables 1-3.

The temperature of the sample was measured by direct measurement of each sample (suspension) in the middle of the drying stage using a non-contact thermometer (PT-7LD, obtained by OPTEX CO., LTD).

The measurement results of samples No. 1-7 are shown in figures 3A-3G, respectively. In figures 3A-3G, the term "cooling" refers to a sample obtained by blowing cold air (10 ° C) over the suspension before the drying step and cooling to about 20 ° C, while the term "without cooling" refers to a sample obtained by watering the suspension and immediately drying without cooling. The results of figures 3A-3G show that cooling the suspension does not affect the temperature of each sample during the drying step.

In sample No. 1, the following hot air drying conditions were used: at a hot air temperature of 70 ° C for 4 minutes, at a hot air temperature of 80 ° C for 4 minutes, and at a hot air temperature of 120 ° C for 4 minutes. The temperature of the sample increased after increasing the temperature of hot air. Finally, it exceeded 100 ° C and reached approximately 120 ° C (Figure 3A). As shown, the "menthol content after storage" of the sheet of sample No. 1 was only 13.6% (table 1). It is assumed that the internal structure of the sheet is destroyed at a high temperature of the sample and, thus, the menthol content after storage is reduced.

In sample No. 2, the following hot air drying conditions were used: at a hot air temperature of 120 ° C for 2 minutes, at a hot air temperature of 130 ° C for 2 minutes, and at a hot air temperature of 176 ° C for 2 minutes. The temperature of the sample increased after increasing the temperature of hot air. Finally, it exceeded 100 ° C and reached approximately 140 ° C (Figure 3B). As shown, the "menthol content after storage" of the sheet of sample No. 2 was only 29.2% (table 1). It is assumed that the internal structure of the sheet is destroyed at a high temperature of the sample and, thus, the menthol content after storage is reduced.

In sample No. 3, hot air drying was used at a hot air temperature of 70 ° C for 60 minutes as a hot air drying condition. Figure 3C shows the temperature of the sample from the start of drying to 14 minutes after drying. The temperature of the sample did not exceed 70 ° C for the duration of the entire drying. As shown, the "menthol content after storage" of the sheet of sample No. 3 was up to 59.2% (table 1). It is assumed that the sheet of sample No. 3 did not reach a high temperature for the duration of the entire drying, and thus, a high menthol content can be maintained after storage under forced conditions. However, sample sheet No. 3 was dried at a sample temperature of less than 70 ° C, and thus 60 minutes were required for drying.

In sample No. 4, the following hot air drying conditions were used: at a hot air temperature of 120 ° C for 5 minutes and at a hot air temperature of 70 ° C for 2.5 minutes. The temperature of the sample reached up to 95 ° C at a hot air temperature of 120 ° C and decreased to 72 ° C at a hot air temperature of 70 ° C (Figure 3D). As shown, the "menthol content after storage" of the sheet of sample No. 4 was up to 62.4% (table 1). It is assumed that the sheet of sample No. 4 was kept at a sample temperature lower than the temperature of samples No. 1 and 2 for the duration of the entire drying process, and thus, a high menthol content can be maintained after storage under forced conditions.

In sample No. 5, the following hot air drying conditions were used: at a hot air temperature of 120 ° C for 4 minutes and at a hot air temperature of 70 ° C for 8 minutes. The temperature of the sample reached up to 95 ° C at a hot air temperature of 120 ° C and decreased to 70 ° C at a hot air temperature of 70 ° C (Figure 3E). As shown, the "menthol content after storage" of the sheet of sample No. 5 was up to 58.5% (table 2). It is assumed that the sheet of sample No. 5 was kept at a temperature of the sample less than the temperature of samples No. 1 and 2 for the duration of the entire drying and, thus, a high menthol content can be maintained after storage under forced conditions.

In sample No. 6, the following hot air drying conditions were used: at a hot air temperature of 110 ° C for 2.2 minutes, at a hot air temperature of 100 ° C for 4.4 minutes and at a hot air temperature of 80 ° C for 2, 2 minutes. The temperature of the sample was maintained in the range of about 80-90 ° C (Figure 3F). As shown, the "menthol content after storage" of the sheet of sample No. 6 was up to 59.9% (table 3). It is assumed that the sheet of sample No. 6 was kept at a sample temperature lower than the temperature of samples No. 1 and 2 for the duration of the entire drying process, and thus, it is possible to maintain a high menthol content after storage under forced conditions.

In sample No. 7, drying with hot air at a temperature of hot air of 100 ° C for 8.8 minutes was used as the conditions for drying with hot air. The temperature of the sample was maintained in the range of approximately 80-90 ° C (Figure 3G). As shown, the "menthol content after storage" of the sheet of sample No. 7 was up to 60.8% (table 3). It is assumed that the sheet of sample No. 7 was kept at a sample temperature lower than the temperature of samples No. 1 and 2 for the duration of the entire drying process, and thus, it is possible to maintain a high menthol content after storage under forced conditions.

The above results show that if the suspension is dried at a sample temperature that does not exceed 100 ° C for the duration of the entire drying process, then a high “menthol content after storage” can be maintained. In addition, it was found that if the suspension is dried at a sample temperature of 70-100 ° C for the duration of the entire drying (except for the period of approximately 1 minute at the beginning of drying), a menthol-containing sheet can be obtained in a shorter time.

[Example 6]

This example shows that cooling the suspension before the drying step affects the “menthol content after storage” of menthol-containing sheets. Specifically, sheets of samples No. 1-7 were obtained as described in examples 1-3. In each of the sheets of samples No. 1-7, the "menthol content after storage" of the sheet obtained by cooling the suspension was compared with the "menthol content after storage" of the sheet obtained without cooling the suspension. As described in Example 1, each sheet was stored in a thermostat set at 50 ° C for 7, 14, and 30 days.

The measurement results of samples No. 1-3 are shown in figure 4A and the measurement results of samples No. 4-7 are shown in the figure. 4B. In figures 4A and 4B, the term "cooling" refers to a sample obtained by blowing cold air (10 ° C) over the suspension before the drying step and cooling to approximately 20 ° C, while the term "without cooling" refers to a sample obtained by watering the suspension and immediately drying without cooling. In the samples “without cooling”, the temperature of the suspension was not less than 50 ° C during the irrigation and drying of the suspension.

The "cooling" data in figures 4A and 4B are the same as the data in figure 1.

In the sheets of samples No. 1 and 2, the menthol content after storage for 30 days was low, not reaching 30%, regardless of the presence or absence of cooling.

In the sheets of sample No. 3, the menthol content after storage for 30 days was greater than 50%, regardless of the presence or absence of cooling. However, a drying time of 60 minutes was necessary to obtain a sheet of sample No. 3.

In sheets of sample No. 4, the menthol content after storage for 30 days was reduced to 18% in the case of “without cooling”, while the menthol content after storage for 30 days was kept equal to 62% in the case of “cooling”.

In sheets of sample No. 5, the menthol content after storage for 30 days was reduced to 20% in the case of “without cooling”, while the menthol content after storage for 30 days was kept equal to 59% in the case of “cooling”.

In sheets of sample No. 6, the menthol content after storage for 30 days was reduced to 20% in the case of “without cooling”, while the menthol content after storage for 30 days was kept equal to 60% in the case of “cooling”.

In sheets of sample No. 7, the menthol content after storage for 30 days was reduced to 12% in the case of “without cooling”, while the menthol content after storage for 30 days was kept equal to 61% in the case of “cooling”.

The above results show that when a suspension of raw material is cooled once and dried at a sample temperature of 70-100 ° C to obtain a menthol-containing sheet, it is possible to obtain a sheet in a shorter time and maintain a high menthol content after storage.

[Example 7]

In this example, the relationship between the cooling temperature of the suspension and the “initial menthol content” of menthol-containing sheets was investigated. Specifically, for the sheet of sample No. 6 described in Example 3, the cooling temperature of the suspension was changed to 20 ° C, 30 ° C, 40 ° C, 50 ° C and 60 ° C, and various sheets were obtained. The menthol content of the sheet was measured immediately after preparation, i.e., “initial menthol content”.

The measurement results are shown in figure 5. From the results of figure 5, it was observed that the menthol content of the sheet increases as the cooling temperature decreases. Specifically, the sheets showed the following initial menthol content: 64% at a cooling temperature of 20 ° C, 61% at a cooling temperature of 30 ° C, 57% at a cooling temperature of 40 ° C, 52% at a cooling temperature of 50 ° C and 43% at a cooling temperature 60 ° C.

In Example 4, described above, it was shown that the suspension formed a gel at a cooling temperature of 40 ° C. or less, and that when the suspension containing the polysaccharide was cooled and a gel formed, it was difficult to return the suspension to a colloidal state, even if the temperature was subsequently raised. In addition, it is well known that if the temperature of the emulsion is less than 0 ° C, the emulsion freezes and breaks.

Based on these results, it was found that the cooling temperatures are preferably 0-40 ° C, more preferably 0-30 ° C.

[Example 8]

In this example, the relationship between the moisture content of menthol-containing sheets and the percent retention of menthol flavor was investigated. Specifically, for the sheet of sample No. 6 described in example 3, the total drying time of the suspension was changed to 8.16 minutes, 7.92 minutes, 7.64 minutes, 7.44 minutes and 7.08 minutes by increasing the feed speed of the tape in the installation for drying with hot air and received sheets having different moisture content. The moisture content of the obtained sheets was measured. The production conditions and moisture content of the sheets are shown in table 4 below.

Table 4 Sample No. 8-1 8-2 8-3 8-4 8-5 Belt feed rate 1.13 m / min 1.07 m / min 1.04 m / min 1.01 m / min 0.98 m / min Total drying time 7.08 min 7.44 min 7.64 min 7.92 min 8.16 min Moisture content after drying 22.6% by weight 14.6% by weight 11.2% by weight 8.6% by weight 6.1% by weight

The resulting sheets were stored in a thermostat set at 50 ° C for 30 days, as described in example 1. The menthol content was measured for sheets immediately after receipt and sheets after storage. The measurement results are shown in table 5 below as the "initial menthol content" and "the menthol content of the sheets immediately after receipt." The percentage of menthol flavoring was calculated from the menthol content using the equation below.

The percentage of menthol flavoring (%) = {(menthol content after storage) / (initial menthol content)} × 100

The results are shown in figure 6 as "forced storage immediately after receipt".

In addition, the sheets were left for 2 months after receipt, and they were stored in a thermostat set at 50 ° C for 30 days, as described in example 1. The menthol content was measured for sheets immediately after receipt and sheets after storage. The measurement results are shown in table 5 below as the "initial menthol content" and "menthol content of the sheets stored for 2 months after receipt." The percent retention of menthol flavor was calculated by the above equation. The results are shown in figure 6 as "forced storage 2 months after receipt".

Table 5 Sample No. 8-1 8-2 8-3 8-4 8-5 Moisture content after drying 22.6% by weight 14.6% by weight 11.2% by weight 8.6% by weight 6.1% by weight Initial Menthol Content 51.0% 56.5% 59.5% 62.2% 61.0% Menthol content of stored sheets immediately upon receipt 3.0% 35.6% 51.9% 56.3% 56.8% Menthol content of stored sheets 2 months after receipt 3.9% 4.4% 18.1% 50.2% 56.8%

The menthol content of the sheets immediately after preparation was approximately 50-60% in all cases of samples No. 8-1 to 8-5.

In experiments in which the sheets immediately after preparation were stored under forced conditions, the following results were shown: a sheet (sample No. 8-5) having a moisture content of approximately 6% had a percent menthol flavor of 93%, sheet (sample No. 8-4) having a moisture content of approximately 9%, had a percent menthol retention rate of 90%, a sheet (sample No. 8-3) having a moisture content of approximately 11%, had a percent menthol retention of 87%, sheet (sample No. 8-2) having moisture content of approximately 1 5%, had a percent menthol flavor of 63%, and a sheet (sample No. 8-1) having a moisture content of about 23% had a percent menthol flavor of 6%.

In the experiments in which the sheets after receipt were stored under forced conditions 2 months after receipt, the following results were shown: a sheet (sample No. 8-5) having a moisture content of approximately 6% had a percent menthol flavor of 95%, sheet (sample No. 8-4) having a moisture content of approximately 9%, had a percent menthol flavor of 87%, sheet (sample No. 8-3), having a moisture content of approximately 11%, had a menthol flavor of 32%, sheet (sample No. 8- 2) having a moisture content of blizitelno 15%, had a percentage retention of menthol flavor 8%, and a sheet (sample № 8-1), having a moisture content of about 23%, had a menthol flavor preservation percentage of 8%.

These results show that if the moisture content of the sheet becomes high, the percentage of menthol flavoring is unexpectedly reduced, and thus, the sheet is preferably dried so that the moisture content of the sheet is less than 10%, preferably 9% or less. In particular, it was found that even if the sheet is additionally stored under forced conditions 2 months after receipt, it is possible to maintain a high percentage of menthol flavoring by reducing the moisture content of the sheet to about 9% or less.

When the moisture content of the leaf is reduced to less than 3%, the percent retention of the menthol flavor is excellent. However, in this case, “cracking” or “delamination” is observed on the sheet. Thus, the moisture content of the sheet after drying is preferably 3% or more.

[Example 9]

In this example, the effect of the polysaccharide type on the menthol content after storage of menthol-containing sheets was investigated. The polysaccharide used was carrageenan, gellan gum, pectin and konjak-glucomannan.

9-1. Method (temperature-sensitive characteristics of the sol-gel transition)

In this experiment, temperature-sensitive characteristics of the sol-gel transition of each aqueous polysaccharide solution were investigated.

(1) Aqueous solution of carrageenan

water 0.1 l

κ-carrageenan (CARRAGEENAN CS-530 / San-Ei Gen F.F.I., Inc.) 5 g

(2) Aqueous solution of gellan gum

As described in example 4.

(3) Pectin Aqueous Solution

water 0.1 l

pectin (for chemical use, derived from citrus fruits, Wako Pure 15 Chemical Industries, Ltd.) 3 g

(4) Aqueous solution of konjak-glucomannan

water 0.1 l

Konjak-glucomannan (Konjak raw material commerce & industry cooperative society in Gunma prefecture) 1 g

An aqueous polysaccharide solution having the above composition was prepared according to the method of Example 4.

The temperature of the aqueous polysaccharide solution was reduced to 25 ° C. over approximately 900 seconds. Then, the temperature was raised for approximately 900 seconds. Changes in the viscosity (fluidity) of an aqueous polysaccharide solution after lowering and increasing temperature were measured with a rheometer (RheoStress 1, obtained by Thermo-Haake). The results of an aqueous solution of carrageenan are shown in figures 7A and 7B, the results of an aqueous solution of gellan gum are shown in figures 2A and 2B, the results of an aqueous solution of pectin are shown in figures 7G and 7H, and the results of an aqueous solution of konjac-glucomannan are shown in figures 7K and 7L.

9-2. Results (temperature-sensitive characteristics of the sol-gel transition)

As shown in Figure 7A, if the temperature of the aqueous carrageenan solution was reduced to 25 ° C, the viscosity became low (approximately 1000 mPa · s or less) up to a temperature of approximately 50 ° C, which was the temperature of the sol to gel transition. However, the viscosity unexpectedly increased at a temperature lower than the transition temperature, and the viscosity reached 10,000,000 mPa · s (gelation). As shown in FIG. 7B, if the temperature of the obtained gel was increased, the gel did not easily return to the colloidal state, even if it was heated at a temperature exceeding the transition temperature. Thus, a gel state can be maintained.

As shown in figures 2A and 2B, when cooling an aqueous solution of gellan gum and the formation of a gel, it is difficult to return to a colloidal state, even if it is heated at a temperature exceeding the transition temperature subsequently. Thus, it is possible to maintain a gel state (see example 4).

As described above, an aqueous solution of carrageenan and an aqueous solution of gellan gum have "temperature-sensitive sol-gel transition characteristics."

On the other hand, the pectin aqueous solution did not have “temperature-sensitive sol-gel transition characteristics”, as shown in Figures 7G and 7H.

In addition, the aqueous solution of konjak-glucomannan did not have "temperature-sensitive characteristics of the sol-gel transition", as shown in figures 7K and 7L.

9-3. Method (receiving sheet)

In this experiment, menthol-containing sheets were prepared using each of the aqueous polysaccharide solutions, and the temperature of the samples was measured during the heat-drying step.

The sheet was prepared according to the same method as in Example 1.

(1) Preparation of Carrageenan-Containing Sheet

Water 10 L

κ-carrageenan (CARRAGEENAN CS-530 / San-Ei Gen F.F.I., Inc.) 500 g

5% aqueous lecithin solution (SUN LECITHIN A-l, Taiyo Kagaku Co., Ltd.) 200 ml

Menthol (Takasago International Corporation.) 2500 g

500 g (5 parts by weight) of κ-carrageenan was added to 10 L (100 parts by weight) of water (heated and aged at 80 ° C) and dissolved in small portions so that no lumps formed (required time: approximately 20 minutes ), while mixing them with a mixer (PRIMIX TK AUTO MIXER Model 40 / equipped with a rotor for mixing the solution / 2000 rpm). 2500 g (25 parts by weight) of l-menthol were added at the same temperature. The rotating blade stirrer was replaced with a homogenizer (PRIMIX T.K. AUTO MIXER Model 40 / equipped with a rotor-stator head / 4000 rpm), and the mixture was emulsified for 10 minutes. Then, 200 ml (2 parts by weight) of a 5% aqueous lecithin solution was added to it, and they were mixed. Menthol was dispersed in an aqueous solution of carrageenan.

The dispersed suspension was poured onto a substrate (PET film, FE2001, FUTAMURA CHEMICAL CO., LTD.) So as to obtain a thickness of 1 mm (wet). Then, the suspension was cooled to approximately 20 ° C using cold air with a temperature of approximately 10 ° C generated by a local cooler (Suiden SS-25DD-1).

Then, the cooled suspension was dry formed using a hot air dryer according to the same method as in Example 1 so as to obtain a moisture content of approximately 6%, and thereby a carrageenan-containing sheet was obtained. Moisture content was measured by GC-TCD (see example 1). The following hot air drying conditions were used: at a hot air temperature of 110 ° C for 3 minutes, at a hot air temperature of 100 ° C for 6 minutes and at a hot air temperature of 80 ° C for 3 minutes (total drying time: 12 minutes) .

A control sheet (without cooling) was obtained by dry molding the poured suspension without cooling. The hot air drying conditions of the control sheet were as follows: at a hot air temperature of 110 ° C for 2.5 minutes, at a hot air temperature of 100 ° C for 5 minutes, and at a hot air temperature of 80 ° C for 2.5 minutes (total drying time: 10 minutes).

The temperature of the sample was measured using a non-contact thermometer in a manner analogous to the method of example 5. Figure 7C shows the change in temperature of the sample during the drying step. In Figure 7C, “cooling” is a sample that was cooled to about 20 ° C by blowing cold air (10 ° C) above it before the drying step, while “without cooling” is a sample that was dried immediately after watering the suspension without cooling . Figure 7C shows that the cooling of the suspension does not affect the temperature of each sample during the drying step.

(2) Obtaining containing gellan gum sheet

Water 10 L

Gellan Gum (KELCOGEL, San-Ei Gen F.F.I., Inc.) 300 g

5% aqueous lecithin solution (SUN LECITHIN A-l, Taiyo Kagaku Co., Ltd.) 120 ml

menthol (Takasago International Corporation.) 1500 g

300 g (3 parts by weight) gellan gum was added to 10 L (100 parts by weight) of water (heated and aged at 80 ° C) and dissolved in small portions so that no lumps formed (required time: approximately 20 minutes) while stirring them with a mixer (PRIMIX TK AUTO MIXER Model 40 / equipped with a rotor for mixing the solution / 2000 rpm). 1500 g (15 parts by weight) of l-menthol were added at the same temperature. The rotating blade stirrer was replaced with a homogenizer (PRIMIX T.K. AUTO MIXER Model 40 / equipped with a rotor-stator head / 4000 rpm), and the mixture was emulsified for 10 minutes. Then, 120 ml (1.2 parts by weight) of a 5% aqueous lecithin solution was added to it, and they were mixed. Menthol was dispersed in an aqueous solution of gellan gum.

The dispersed suspension was poured onto a substrate (PET film, FE2001, FUTAMURA CHEMICAL CO., LTD.) So as to obtain a thickness of 1 mm (wet). Then, the suspension was cooled to approximately 20 ° C using cold air with a temperature of approximately 10 ° C generated by a local cooler (Suiden SS-25DD-1).

Then, the cooled suspension was dry formed using a hot air dryer according to the same method as in Example 1 so as to obtain a moisture content of approximately 6%, and thereby a gellan gum sheet was obtained. Moisture content was measured by GC-TCD (see example 1). The following hot air drying conditions were used: at a hot air temperature of 110 ° C for 2.8 minutes, at a hot air temperature of 100 ° C for 5.5 minutes and at a hot air temperature of 80 ° C for 2.8 minutes (total drying time: 11 minutes).

A control sheet (without cooling) was obtained by dry molding the poured suspension without cooling. The hot air drying conditions of the control sheet were as follows: at a hot air temperature of 110 ° C for 2.3 minutes, at a hot air temperature of 100 ° C for 4.5 minutes, and at a hot air temperature of 80 ° C for 2.3 minutes (total drying time: 9 minutes).

The temperature of the sample was measured using a non-contact thermometer in a manner analogous to the method of example 5. Figure 7E shows the temperature change of the sample during the drying step. In Figure 7E, “cooling” is a sample that was cooled to about 20 ° C by blowing cold air (10 ° C) above it before the drying step, while “without cooling” is a sample that was dried immediately after watering the suspension without cooling . Figure 7E shows that cooling the suspension does not affect the temperature of each sample during the drying step.

(3) Obtaining a pectin-containing sheet

water 10 l

pectin (chemical use derived from citrus, Wako Pure Chemical Industries, Ltd.) 300 g

5% aqueous lecithin solution (SUN LECITHIN A-l, Taiyo Kagaku Co., Ltd.) 120 ml

Menthol (Takasago International Corporation.) 1500 g

300 g (3 parts by weight) of pectin was added to 10 L (100 parts by weight) of water (heated and aged at 80 ° C) and dissolved in small portions so that no lumps formed (required time: approximately 20 minutes), while stirring them with a mixer (PRIMIX TK AUTO MIXER Model 40 / equipped with a rotor for mixing the solution / 2000 rpm). 1500 g (15 parts by weight) of l-menthol were added at the same temperature. The rotating blade stirrer was replaced with a homogenizer (PRIMIX T.K. AUTO MIXER Model 40 / equipped with a rotor-stator head / 4000 rpm), and the mixture was emulsified for 10 minutes. Then, 120 ml (1.2 parts by weight) of a 5% aqueous lecithin solution was added to it, and they were mixed. Menthol was dispersed in an aqueous pectin solution.

The dispersed suspension was poured onto a substrate (PET film, FE2001, FUTAMURA CHEMICAL CO., LTD.) So as to obtain a thickness of 1 mm (wet). Then, the suspension was cooled to approximately 20 ° C using cold air with a temperature of approximately 10 ° C generated by a local cooler (Suiden SS-25DD-1).

Then, the cooled suspension was dry formed using a hot air dryer according to the same method as in Example 1 so as to obtain a moisture content of approximately 6%, and thereby a pectin-containing sheet was obtained. Moisture content was measured by GC-TCD (see example 1). The following hot air drying conditions were used: at a hot air temperature of 110 ° C for 2.8 minutes, at a hot air temperature of 100 ° C for 5.5 minutes and at a hot air temperature of 80 ° C for 2.8 minutes (total drying time: 11 minutes).

A control sheet (without cooling) was obtained by dry molding the poured suspension without cooling. The hot air drying conditions of the control sheet were as follows: at a hot air temperature of 110 ° C for 2.5 minutes, at a hot air temperature of 100 ° C for 5 minutes, and at a hot air temperature of 80 ° C for 2.5 minutes (total drying time: 10 minutes).

The temperature of the sample was measured using a non-contact thermometer in a manner analogous to the method of example 5. Figure 7I shows the temperature change of the sample during the drying stage. In figure 7I, “cooling” is a sample that was cooled to about 20 ° C by blowing cold air (10 ° C) above it before the drying step, while “without cooling” is a sample that was dried immediately after watering the suspension without cooling . Figure 7I shows that cooling the suspension does not affect the temperature of each sample during the drying step.

(4) Preparation of konjac-glucomannan-containing sheet

Water 10 L

Konjak-glucomannan (Konjak raw material commerce & industry cooperative society in Gunma prefecture) 100 g

5% aqueous lecithin solution (SUN LECITHIN A-1, Taiyo Kagaku Co., Ltd.) 40 ml

menthol (Takasago International Corporation.) 500 g

100 g (1 part by weight) of konjak-glucomannan was added to 10 l (100 parts by weight) of water (heated and aged at 80 ° C) and dissolved in small portions so that no lumps formed (required time: approximately 20 minutes ), while mixing them with a mixer (PRIMIX TK AUTO MIXER Model 40 / equipped with a rotor for mixing the solution / 2000 rpm). 500 g (5 parts by weight) of l-menthol was added at the same temperature. The rotating blade stirrer was replaced with a homogenizer (PRIMIX T.K. AUTO MIXER Model 40 / equipped with a rotor-stator head / 4000 rpm), and the mixture was emulsified for 10 minutes. Then, 40 ml (0.4 parts by weight) of a 5% aqueous lecithin solution was added to it, and they were mixed. Menthol was dispersed in an aqueous solution of konjak-glucomannan.

The dispersed suspension was poured onto a substrate (PET film, FE2001, FUTAMURA CHEMICAL CO., LTD.) So as to obtain a thickness of 1 mm (wet). Then, the suspension was cooled to approximately 20 ° C using cold air with a temperature of approximately 10 ° C generated by a local cooler (Suiden SS-25DD-1).

Then, the cooled suspension was dry formed using a hot air dryer according to the same method as in Example 1 so as to obtain a moisture content of approximately 6%, and thereby a konjac-glucomannan-containing sheet was obtained. Moisture content was measured by GC-TCD (see example 1). The following hot air drying conditions were used: at a hot air temperature of 110 ° C for 3 minutes, at a hot air temperature of 100 ° C for 6 minutes and at a hot air temperature of 80 ° C for 3 minutes (total drying time: 12 minutes) .

A control sheet (without cooling) was obtained by dry molding the poured suspension without cooling. The hot air drying conditions of the control sheet were as follows: at a hot air temperature of 110 ° C for 2.5 minutes, at a hot air temperature of 100 ° C for 5 minutes, and at a hot air temperature of 80 ° C for 2.5 minutes (total drying time: 10 minutes).

The temperature of the sample was measured using a non-contact thermometer in a manner analogous to the method of example 5. Figure 7M shows the temperature change of the sample during the drying step. In Figure 7M, “cooling” is a sample that was cooled to about 20 ° C by blowing cold air (10 ° C) above it before the drying step, while “without cooling” is a sample that was dried immediately after watering the suspension without cooling . Figure 7M shows that cooling the suspension does not affect the temperature of each sample during the drying step.

9-4. Method (measuring menthol)

The menthol content of the sheet was measured immediately after preparation (initial menthol content) and the menthol content of the sheet stored under forced conditions (menthol content after storage). The forced conditions were as described in Example 1. The menthol content was measured according to the same method as in Example 1. The results for the carrageenan-containing sheet are shown in Figure 7D, the results for the gellan gum-containing sheet were shown in Figure 7F, the results for the pectin-containing sheet shown in FIG. 7J and the results for a konjac-glucomannan containing sheet are shown in FIG. 7N.

9-5. Results (menthol content)

In the case of a carrageenan-containing sheet, as shown in FIG. 7D, when the suspension was cooled before the drying step, the initial menthol content was approximately 80% by weight, and the menthol content after storage for 30 days was 60% by weight or more (percentage of menthol flavoring = approximately 80%). On the other hand, when the suspension was not cooled before the drying step, the initial menthol content was approximately 80% by weight, and the menthol content after storage for 30 days was approximately 45% by weight (percent retention of menthol flavor = approximately 60%).

In the case of gellan gum-containing sheet, as shown in FIG. 7F, when the suspension was cooled before the drying step, the initial menthol content was approximately 70% by weight, and the menthol content after storage for 30 days was approximately 65% by weight (percentage of menthol flavoring = approximately 90% or more). On the other hand, when the suspension was not cooled before the drying step, the initial menthol content was approximately 55% by weight, and the menthol content after storage for 30 days was approximately 35% by weight (percent retention of menthol flavor = approximately 65%).

In the case of a pectin-containing sheet, as shown in FIG. 7J, whether or not the suspension was cooled before the drying step, the initial menthol content was approximately 60% by weight, and the menthol content after storage for 30 days was approximately 30% by weight ( percent retention of menthol flavoring = from about 55% to about 65%).

In the case of a konjac-glucomannan containing sheet as shown in FIG. 7N, whether or not the suspension was cooled before the drying step, the initial menthol content was approximately 30% by weight and the menthol content after storage for 30 days was approximately 15% by weight (percent retention of menthol flavor = approximately 50%).

The above results show that when carrageenan or gellan gum is used as a polysaccharide and the suspension is cooled before the drying step, and then dried, the resulting sheet has a high menthol content and a high menthol yield, and also maintains a high menthol content after storage.

Therefore, in the following examples, carrageenan or gellan gum was used as a polysaccharide, and the suspension was cooled before the drying step, and then dried.

[Example 10]

In this example, the effect of polysaccharide concentration on the menthol content after storage of menthol-containing sheets was investigated.

10-1. Method (temperature-sensitive characteristics of the sol-gel transition)

In this experiment, the temperature-sensitive characteristics of the transition of the sol to the gel of suspensions of the raw material (solution for producing the sheet) containing the polysaccharide at various concentrations were investigated. The polysaccharide used was 1 part by weight (1%), 2 parts by weight (2%), 3 parts by weight (3%), 5 parts by weight (5%) and 7 parts by weight (7%) of carrageenan relative to water (100 parts by weight). In addition, 1 part by weight (1%), 2 parts by weight (2%), 3 parts by weight (3%), 5 parts by weight (5%) and 7 parts by weight (7%) gellan gum were used relative to water (100 parts by weight). In the following description and figures 8A-8F, the polysaccharide concentration is presented as a percentage by weight (%) relative to water.

Suspensions of raw material containing carrageenan and suspensions of raw material containing gellan gum were prepared as described in column 9-3 of Example 9. Depending on the polysaccharide concentrations, menthol was added in 5-fold relative to the polysaccharide (weight ratio), and 5% aqueous a solution of lecithin was added in an amount of two fifths relative to the polysaccharide (weight ratio).

The temperature of the suspensions of the raw material containing polysaccharides at various concentrations was reduced from 70 ° C to 25 ° C for approximately 900 seconds. Then, the temperature was raised to 70 ° C for approximately 900 seconds. Changes in the viscosity (flow) of suspensions after lowering and increasing temperature were measured with a rheometer (RheoStress 1, obtained by Thermo-Haake). The results for the carrageenan-containing suspension are shown in Figures 8A and 8B, and the results for the gellan gum-containing suspension are shown in Figures 8D and 8E.

10-2. Results (temperature-sensitive characteristics of the sol-gel transition)

As shown in figures 8A and 8B, in the case of a suspension of raw material containing 1% by weight of carrageenan, even if the suspension was cooled to 25 ° C, it was not sufficiently gelled. When the temperature of this raw material was increased subsequently, it was difficult to maintain a gel state. In the case of a suspension of raw material containing 7% by weight of carrageenan, the viscosity increased at an early stage of the temperature lowering process (from 70 to 60 ° C), and it was difficult to maintain a colloidal state. Accordingly, it was difficult to disperse menthol during the preparation of a given suspension of crude material.

Therefore, it is preferable that carrageenan is contained in a suspension of crude material at a concentration of 2-5% by weight.

As shown in figures 8D and 8E, in the case of a suspension of raw material containing 1% by weight of gellan gum, even if the suspension was cooled to 25 ° C, it was not sufficiently gelled. When the temperature of this raw material was increased subsequently, it was difficult to maintain a gel state. In the case of a suspension of raw material containing 7% by weight of gellan gum, the viscosity increased at an early stage in the process of lowering the temperature (from 70 to 60 ° C), it was difficult to maintain a colloidal state. Accordingly, it was difficult to disperse menthol during the preparation of this suspension of crude material.

Therefore, it is preferable that gellan gum is contained in a suspension of raw material at a concentration of 2-5% by weight.

10-3. Method (obtaining a sheet and measuring menthol content)

Carrageenan-containing sheets and gellan gum-containing sheets were prepared using raw material suspensions containing polysaccharides at various concentrations (see column 10-1). The sheet was prepared according to the same method as in Example 9.

The menthol content of the sheet was measured immediately after preparation (initial menthol content) and the menthol content of the sheet stored under forced conditions (the menthol content after storage). The forced conditions were as described in Example 1. The menthol content was measured according to the same method as in Example 1. The results for the carrageenan-containing sheet are shown in Figure 8C, and the results for the gellan gum-containing sheet were shown in Figure 8F.

10-4. Results (menthol content)

In any case, with 3% by weight or 5% by weight of a carrageenan-containing sheet, as shown in FIG. 8C, the initial menthol content was approximately 80% by weight, and the menthol content after storage for 30 days was approximately 60% by weight ( percent retention of menthol flavor = approximately 80%). In the case of 2% by weight of carrageenan, the initial menthol content was 74% by weight, and the menthol content after storage for 30 days exceeded 50% by weight (percentage of menthol flavoring = 68%). In the case of 6% by weight of carrageenan, the initial menthol content was 69% by weight, and the menthol content after storage for 30 days was 43% by weight (percent retention of menthol flavor = 62%).

In any case, with 3% by weight or 5% by weight of gellan gum-containing sheet, as shown in Figure 8F, the initial menthol content was approximately 70% by weight, and the menthol content after storage for 30 days was close to 70% by weight. weight (percent retention of menthol flavor = approximately 90%). In the case of 2% by weight of gellan gum, the initial menthol content was approximately 70% by weight, and the menthol content after storage for 30 days exceeded 50% by weight (percent retention of menthol flavor = 78%). In the case of 6% by weight of gellan gum, the initial menthol content was 76% by weight, and the menthol content after storage for 30 days was 63% by weight (percent retention of menthol flavor = 83%).

These results show that carrageenan or gellan gum is contained in a suspension of raw material at a concentration of preferably 2-6% by weight, more preferably 3-5% by weight.

[Example 11]

In this example, the effect of the proportion of menthol contained in the slurry of the crude material on the menthol content after storage and the menthol yield of menthol-containing sheets was investigated.

11-1. Method (obtaining a sheet and measuring menthol content)

Carrageenan-containing sheets and gellan gum-containing sheets were prepared using raw material suspensions containing various proportions in a menthol mixture. The sheet was prepared according to the same method as in Example 9.

As for the sheets containing carrageenan, menthol was added in an amount equivalent to 1, 2.5, 5, 10, 15, and 20 times the weight of 5% by weight of carrageenan (in a suspension of raw material). As for the gellan gum-containing sheets, menthol was added in an amount equivalent to 0.5, 1, 2.5, 5, 10, 15 and 20 times the weight of 3% by weight of gellan gum (in a suspension of raw material).

The menthol content of the sheet was measured immediately after preparation (initial menthol content) and the menthol content of the sheet stored under forced conditions (the menthol content after storage). The forced conditions were as described in Example 1. The menthol content was measured according to the same method as in Example 1. The results for the carrageenan-containing sheet are shown in Figures 9A-9E, and the results for the gellan gum-containing sheet were shown in Figures 9F-9J. In these figures, the expression [1: x] represents the weight ratio of polysaccharide and menthol in a suspension of raw material. For example, the expression [1: 5] represents that menthol is contained in a suspension of crude material in an amount equivalent to 5 times the weight of the polysaccharide. In these figures, the term "immediately after receipt" refers to the sheet immediately after receipt, and the term "after 1 month at 50 °" refers to the sheet after storage at 50 ° C for 30 days.

11-2. results

(1) Carrageenan-containing sheet

As for the carrageenan-containing sheets, as shown in FIG. 9A, the “initial menthol content” was the highest in the case of the sheet containing menthol in 10 times the weight, the second largest in the case of the sheet containing menthol in 5 times the weight , the third largest in the case of a sheet containing menthol in a 2.5-fold amount by weight, and the fourth largest in the case of a sheet containing menthol in a 1-fold amount in weight. These results showed that the initial menthol content depended on the proportion of menthol in the mixture. On the other hand, in the case of sheets containing menthol in 15-fold and 20-fold amounts by weight, the “initial menthol content” was only 20% by weight or less. In all cases, the proportion of menthol in the mixture, the "menthol content after storage" is extremely slightly reduced relative to the initial menthol content. Thus, as shown in FIG. 9B, the percent retention of the menthol flavor after storage for 30 days exceeded 70% in all cases, fractions in the menthol mixture. Among them, a leaf containing menthol in a 2.5-fold amount by weight possessed a percentage of menthol flavor of approximately 100%.

The ratio of the menthol content in the sheet to the proportion of menthol added to the slurry of the crude material was calculated as “menthol yield (%)” using the equation below.

The menthol yield (%) = {(measured value of the menthol content in the sheet) / (proportion in the menthol mixture)} × 100

As shown in FIG. 9C, the “menthol yield” immediately after receiving the sheet showed a value in excess of 50% in all cases of samples in which the proportion in the menthol mixture was 1-10-fold by weight. The “menthol yield” after storage showed the highest value in the case of a sheet containing menthol in a 2.5-fold amount by weight. A sheet containing menthol in a 5-fold or 10-fold amount by weight showed a lower "menthol yield" after storage than a sheet containing menthol in a 2.5-fold amount by weight, but the menthol content in the sheet (absolute amount) was large (see figure 9A).

Figures 9D and 9E show the relationship between the fraction in the mixture (%) of menthol and the menthol content (%) and the relationship between the proportion in the mixture (%) of menthol and the yield of menthol (%), respectively. In these figures, the fraction in the menthol mixture (%) is represented by the formula: {fraction in the menthol mixture / (fraction in the menthol mixture + fraction in the carrageenan mixture)} × 100.

As shown in FIG. 9D, sheets in which the proportion in the menthol mixture was 2.5-10 times by weight (i.e., the proportion in the menthol mixture was 71-91%) showed a high menthol content after storage. As shown in FIG. 9E, sheets in which the proportion in the menthol mixture was 1-5 times by weight (i.e., the proportion in the menthol mixture was 50-83%) showed a high menthol yield after storage.

The results of figures 9A to 9E show that the proportion in the menthol mixture relative to carrageenan is preferably 1-10 times the amount by weight, more preferably 2.5-5 times the amount by weight.

(2) Gellan Gum Sheet

For gellan gum-containing sheets, as shown in FIG. 9F, the “initial menthol content” was greatest for a sheet containing menthol in 5-fold by weight, smallest in the case of sheet containing menthol in 0.5-fold by weight , and depends on the proportion in the mixture of menthol in the sheets, in which the proportion in the mixture of menthol was 0.5-5 times the amount by weight. In samples in which the proportion of menthol in the mixture was 0.5-5 times by weight, the “menthol content after storage” decreased very slightly relative to the initial menthol content. However, in sheets in which the proportion of menthol in the mixture was 10-fold by weight or more, the menthol content decreased with increasing storage days. Thus, as shown in Figure 9G, the percentage of menthol flavor after storage for 30 days exceeded 90% in sheets in which the proportion in the menthol mixture was 0.5-5 times by weight. However, the percent retention of menthol flavor was approximately 50% in the sheets, in which the proportion in the menthol mixture was 10 times the amount by weight or more. As described above, sheets in which the proportion in the menthol mixture was 0.5-5 times by weight had a high percentage of menthol flavor retention. Among them, a leaf containing menthol in a 2.5-fold amount by weight had a menthol flavor percentage of approximately 100%.

As shown in Figure 9H, the “menthol yield” immediately after receiving the sheet showed a value exceeding 50% in the case of sheets containing menthol in 1-, 2.5-, and 5-fold amounts by weight. The "menthol yield" after storage was the highest in the case of a sheet containing menthol in a 2.5-fold amount by weight. A sheet containing menthol in a 5-fold amount by weight had a lower “menthol yield” after storage than a sheet containing menthol in a 2.5-fold amount by weight, but the menthol content in the sheet (absolute amount) is large (see figure 9F).

Figures 9I and 9J show the relationship between the proportion in the mixture (%) of menthol and the menthol content (%) and the relationship between the proportion in the mixture (%) of menthol and the yield of menthol (%), respectively. In the figures, the fraction in the menthol mixture (%) is represented by the formula: {fraction in the menthol mixture / (fraction in the menthol mixture + fraction in the gellan gum mixture)} × 100.

As shown in FIG. 9I, sheets in which the proportion in the menthol mixture was 2.5-5 times by weight (i.e., the proportion in the menthol mixture was 71-83%) had a high menthol content after storage. As shown in FIG. 9J, sheets in which the proportion in the menthol mixture was 1-5 times the weight (i.e., the proportion in the menthol mixture was 50-83%) had a high menthol yield after storage.

The results of figures 9F-9J show that the proportion in the menthol mixture relative to gellan gum is preferably 1-10 times by weight, more preferably 2.5-5 times by weight.

[Example 12]

In this example, the effect of the proportion of lecithin contained in a suspension of raw material on the menthol content after storage of menthol-containing sheets was investigated.

12-1. Method (obtaining a sheet and measuring menthol content)

Carrageenan-containing sheets and gellan gum-containing sheets were prepared using raw material suspensions containing various proportions in a lecithin mixture. The sheet was prepared according to the same method as in Example 9.

For carrageenan-containing sheets, lecithin was added in an amount equivalent to 0.001, 0.005, 0.01, 0.02, 0.05, 0.1, 0.2, and 0.4 times the amount by weight of 5% by weight of carrageenan ( in a suspension of raw material). Menthol was added in an amount equivalent to 5 times the weight of carrageenan.

Similarly, for gellan gum-containing sheets, menthol was added in an amount equivalent to 0.001, 0.005, 0.01, 0.02, 0.05, 0.1, 0.2 and 0.4 times the amount by weight of 3% by weight the weight of gellan gum (in a suspension of raw material). Menthol was added in an amount equivalent to 5 times the weight of gellan gum.

The menthol content of the sheet was measured immediately after preparation (initial menthol content) and the menthol content of the sheet stored under forced conditions (the menthol content after storage). The forced conditions were as described in Example 1. The menthol content was measured according to the same method as in Example 1. The results for the carrageenan-containing sheet are shown in Figures 10A and 10B, and the results for the gellan gum-containing sheet were shown in Figures 10C and 10D. In figures 10A and 10C, the numerical values in braces represent the weight ratios of lecithin relative to the polysaccharide. For example, the expression [0.01] is that lecithin is contained in a suspension of crude material in an amount equivalent to 0.01 times the weight of the polysaccharide. In figures 10B and 10D, the term "immediately after receipt" means a sheet immediately after receipt, and the term "after 1 month at 50 ° C" means a sheet after storage at 50 ° C for 30 days.

12-2. results

(1) Carrageenan-containing sheet

As for the carrageenan-containing sheets, as shown in FIG. 10A, the menthol content was significantly reduced after storage when the proportion in the lecithin mixture relative to carrageenan was 0.1-0.4 times the amount by weight.

Figure 10B shows the relationship between the proportion in the mixture of lecithin (weight ratio relative to carrageenan) and the menthol content (%). As shown in FIG. 10B, a high menthol content was maintained after storage in sheets in which the proportion in the lecithin mixture relative to carrageenan was 0.005-0.02 times the amount by weight.

(2) Gellan Gum Sheet

As for the gellan gum-containing sheets, as shown in FIG. 10C, the menthol content was significantly reduced after storage in the case where the proportion of the lecithin relative to the gellan gum was 0.1-0.4 times by weight.

Figure 10D shows the relationship between the proportion of the lecithin mixture (weight ratio relative to gellan gum) and the menthol content (%). As shown in Figure 10D, a high menthol content was maintained after storage of sheets in which the proportion of lecithin relative to gellan gum was 0.005-0.05 times the amount by weight.

From the results of Figures 10A-10D, it was found that the proportion in the lecithin mixture relative to the polysaccharide is preferably 0.5-5% by weight. Specifically, when carrageenan is used as a polysaccharide, the proportion in the lecithin mixture relative to the polysaccharide is preferably 0.5-2% by weight. When gellan gum is used as a polysaccharide, the proportion of the lecithin mixture relative to the polysaccharide is preferably 0.5-5% by weight, more preferably 0.5-2% by weight.

[Example 13]

In this example, the effect of the type of emulsifier on the menthol content after storage of menthol-containing sheets was investigated.

13-1. Method (obtaining a sheet and measuring menthol content)

Carrageenan-containing sheets and gellan gum-containing sheets were prepared using raw material suspensions containing various types of emulsifiers. The sheet was prepared according to the same method as in Example 9. Menthol was added in an amount equivalent to 5 times the weight of the polysaccharide, and each emulsifier was added in an amount equivalent to 0.02 times the weight of the polysaccharide.

The eight types of emulsifiers below were used as an emulsifier. The numbers 1-8 given to the emulsifiers below correspond to the numbers of figures 11A and 11B.

1. Lecithin

(SUN LECITHIN A-1, obtained by Taiyo Kagaku Co., 10 Ltd.)

2. Fatty acid ester of glycerol (monoglyceride)

(Exel S-95, obtained by Kao Corporation)

Compound name: lipophilic glycerol monostearate

3. Fatty acid ester of glycerol (polyglyceride)

(SunSoft A-181E, obtained by Taiyo Kagaku Co., Ltd.)

Compound Name: Pentaglycerol Monostearate

4. Fatty acid ester of glycerol (organic acid monoglyceride)

(Step SS, obtained by Kao Corporation)

Compound Name: Monoglyceride Succinate

5. Fatty acid ester and sorbitan

(Emasol S-10V, obtained by Kao Corporation)

Compound Name: Sorbitan Monostearate

6. Fatty acid ester and sorbitan (polysorbate)

(Emasol S-120V, obtained by Kao Corporation)

Compound Name: Polyoxyethylene Sorbitan Monostearate

7. Fatty acid ester and propylene glycol

(Sunsoft No. 25CD, obtained by Taiyo Kagaku Co., Ltd.)

Compound Name: Propylene Glycol Monostearate

8. Fatty acid ester and sucrose

(Ryoto sugar ester S-1570, obtained by Mitsubishi-Kagaku Foods Corporation)

Compound name: stearic acid and sucrose ester

The menthol content of the sheet was measured immediately after preparation (initial menthol content) and the menthol content of the sheet stored under forced conditions (the menthol content after storage). The forced conditions were as described in Example 1. The menthol content was measured according to the same method as in Example 1. The results for the carrageenan-containing sheet are shown in Figure 11A, and the results for the gellan gum-containing sheet were shown in Figure 11B. In figures 11A and 11B, the term "immediately after receipt" means the sheet immediately after receipt, and the term "after 1 month at 50 ° C" means the sheet after storage at 50 ° C for 30 days.

13-2. results

The results of figures 11A and 11B show that various emulsifiers can be used in addition to lecithin. For carrageenan-containing sheets, it is particularly preferable to use 1. lecithin, 3. fatty acid ester and glycerol (polyglyceride) and 4. fatty acid ester and glycerin (organic acid monoglyceride) as emulsifiers. As regards sheets containing gellan gum, it is particularly preferable to use 1. lecithin, 2. fatty acid and glycerol ether (monoglyceride), 3. fatty acid and glycerol ether (polyglyceride), 4. fatty acid and glycerol ether (organic monoglyceride), 5 fatty acid ester of sorbitan, 7. fatty acid ester of propylene glycol and 8. fatty acid ester of sucrose as emulsifiers.

Claims (13)

1. A method of obtaining a fragrance-containing sheet for a smoking article, characterized in that it includes:
the step of applying a slurry of raw material to a substrate, where the slurry contains a polysaccharide containing at least one of carrageenan and gellan gum, a flavoring agent, an emulsifier and 70-95% by weight of water, has a flavoring content of 100-1000% by weight relative to the polysaccharide and has a temperature 60-90 ° C in colloidal state;
a step of actively cooling the applied suspension of the crude material to a sample temperature of 0-40 ° C. to obtain a gel; and
the stage of thermal drying, including heating the gelled raw material and drying it at a sample temperature of 70-100 ° C. 2. A method of obtaining a fragrance-containing sheet for a smoking article according to claim 1, characterized in that the emulsifier is 0.5-5% by weight of lecithin relative to the polysaccharide. 3. A method of obtaining a fragrance-containing sheet for a smoking article according to claim 1, characterized in that the emulsifier is an ether selected from the group consisting of a fatty acid ester and glycerol, a fatty acid ester and polyglycerol, a fatty acid ester and sorbitan, an ether fatty acid and propylene glycol; and fatty acid ester and sucrose. 4. The method of obtaining containing a flavoring sheet for a product for smoking according to claim 1, characterized in that the polysaccharide is contained in a suspension of raw material at a concentration of 2-6% by weight. 5. A method of obtaining a flavoring-containing sheet for a smoking article according to claim 1, characterized in that the flavoring is menthol. 6. A method of obtaining a fragrance-containing sheet for a smoking article according to claim 5, characterized in that the menthol content is in the range of 250-500% by weight relative to the polysaccharide. 7. A sheet for a product for smoking, containing a flavoring, characterized in that it is obtained by the method according to any one of claims 1 to 4. 8. Sheet for products for smoking, containing a flavoring, characterized in that it is obtained by the method according to claim 5 or 6. 9. The sheet for a smoking article of claim 8, characterized in that the menthol content of the sheet after receipt is 45% by weight or more, and the menthol content of the sheet after storage at 50 ° C for 30 days is 45% by weight or more . 10. A smoking article containing ground tobacco, characterized in that the cut pieces of the flavoring sheet for the smoking article of claim 7 are mixed with ground tobacco. 11. A smoking article containing ground tobacco, characterized in that the sliced pieces of the flavoring sheet for the smoking article of claim 8 are mixed with ground tobacco. 12. A cigarette containing a cigarette rod that contains crushed tobacco and cigarette paper in which crushed tobacco is wrapped, characterized in that the cut pieces of the flavoring sheet for the smoking article of claim 7 are mixed with crushed tobacco. 13. A cigarette containing a cigarette rod that contains crushed tobacco and cigarette paper in which crushed tobacco is wrapped, characterized in that the cut pieces of the flavoring sheet for a smoking article of claim 8 are mixed with crushed tobacco.

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